CN115434043B - Device and method for pressurizing and not melting asphalt fibers - Google Patents
Device and method for pressurizing and not melting asphalt fibers Download PDFInfo
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- CN115434043B CN115434043B CN202211287381.7A CN202211287381A CN115434043B CN 115434043 B CN115434043 B CN 115434043B CN 202211287381 A CN202211287381 A CN 202211287381A CN 115434043 B CN115434043 B CN 115434043B
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- 238000002844 melting Methods 0.000 title claims abstract description 76
- 230000008018 melting Effects 0.000 title claims abstract description 76
- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 239000010426 asphalt Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001819 mass spectrum Methods 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 26
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 11
- 239000004917 carbon fiber Substances 0.000 abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 238000004949 mass spectrometry Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000005070 sampling Methods 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 11
- 238000001816 cooling Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 3
- 239000011302 mesophase pitch Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/32—Apparatus therefor
- D01F9/322—Apparatus therefor for manufacturing filaments from pitch
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/30—Adapting or protecting infrastructure or their operation in transportation, e.g. on roads, waterways or railways
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a device and a method for pressurizing and not melting asphalt fibers, and belongs to the technical field of asphalt carbon fiber preparation. Aiming at the problems of long oxidation time, low efficiency, environmental pollution and difficult recovery treatment existing in the conventional pitch-based carbon fiber unmelting method, the invention adopts air with constant flow and pressure to unmelt pitch fibers, the pressurizing can promote unmelting reaction to the right, and oxygen in the air can be accelerated to diffuse inwards along the radial direction of the fibers, so that the unmelting time is reduced; on-line detection of H using mass spectrometry 2 O and CO 2 The concentration change of the asphalt fiber is determined, the difficulty of sampling and weighing at a height of Wen Pinfan and determining the degree of the infusible reaction is avoided, so that the defects of long infusible time and complex operation of the asphalt fiber in the prior art are overcome, and the mechanical property of the prepared asphalt fiber is hardly changed compared with that of a conventional air method.
Description
Technical Field
The invention belongs to the technical field of asphalt carbon fiber preparation, and particularly relates to a device and a method for pressurizing and not melting asphalt fibers.
Background
The non-melting is an indispensable important step in the production process flow of the pitch-based carbon fiber, and the mechanical properties of the carbon fiber are directly affected. The asphalt fiber precursor has no strength, is fragile and has thermoplasticity, and the fiber with low heat resistance can be mutually fused, twisted and deformed by directly carbonizing the asphalt fiber precursor, so that the original appearance of the fiber can not be maintained. After non-melting treatment, asphalt molecules in the fiber form a net structure through dehydrogenation, oxidation and crosslinking reaction, become a thermosetting state and release H 2 O、CO 2 And the micromolecular products are equal, so that the carbonized asphalt fiber has certain mechanical strength. The degree of non-melting can also adversely affect the performance of pitch-based carbon fibers; when the degree of non-melting is insufficient, the fiber is easy to form a sheath-core structure, and the fiber is molten and adhered in severe cases; excessive melting degree can cause excessive crosslinking of asphalt molecules, excessive micromolecular decomposition products are released in the carbonization process, so that gaps and cracks in the fiber are increased, defects are formed, and the mechanical properties of the asphalt-based carbon fiber are reduced. Common non-melting methods are two methods, gas and liquid.
The gas-phase unmelting method is to react with active sites of asphalt molecules at a certain temperature using a gas having oxidizing property to generate various oxygen-containing functional groups. Air oxidation is the most common method in pitch-based carbon fiber production, and the oxidizing gas is mainly air, O 2 、O 3 And Cl 2 And the like (CN 112522810A, CN 110284217B, CN 110230127B, CN 105887245A, CN 105088420A, CN 108251919A, CN 110592727A, CN 100529207C, CN 102691135A, CN 102560744A, CN 111020748B, CN 111501134A and CN 102477595A), but the diffusion step is a non-melting block speed step, so that the oxidation time of non-melting at normal pressure is long, the non-melting efficiency is low, and the manufacturing cost of the carbon fiber is further improved. Liquid-phase unmelting is achieved by using oxidizing solutions, e.g. HNO 3 、H 2 SO 4 、H 2 O 2 And the like (CN 103046165A, CN 108486688A, CN 109610047A), which oxidizes the fatty structure of the pitch molecules to oxygen-containing functional groups and crosslinks, wherein the concentration of the solution has a significant effect on the extent to which the pitch fibers do not melt. The disadvantage of the liquid phase not being melted is that waste gas, waste acid are generated, the environment is polluted, the recovery and the treatment are difficult, and the surface of the asphalt fiber can be damaged.
Disclosure of Invention
Aiming at the problems of long oxidation time, low efficiency, environmental pollution and difficult recovery treatment existing in the conventional pitch-based carbon fiber unmelting method, the invention provides a device and a method for pressurizing unmelted pitch fiber.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the device for pressurizing unmelted asphalt fibers is formed by sequentially connecting a mass flowmeter (1), a front constant pressure valve (2), an unmelting furnace (4), an unmelting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7);
further, the mass flowmeter (1), the front constant pressure valve (2), the unmelted reactor (5) and the rear constant pressure valve (4) are connected by stainless steel pipes in sequence; the non-melting reactor (5) is arranged in the tubular heating furnace (4); the sample inlet of the mass spectrum (7) is arranged in the pipeline at the rear end of the rear constant pressure valve (6).
Further, the non-melting furnace (4) is a tubular heating furnace, and a heater capable of programming temperature is arranged on the outer side of the non-melting furnace; the non-melting reactor (5) is a stainless steel reactor, and both ends of the non-melting reactor are sealed hard.
Further, the front constant pressure valve (2) is a constant pressure valve for controlling the pressure of a rear device thereof, preferably a YT-2 type constant pressure valve; the rear constant pressure valve (6) is a constant value, preferably a YT-4 type constant pressure valve, for controlling the pressure of a front device.
A method of pressurizing a non-melting pitch fiber apparatus to non-melt pitch fibers, comprising the steps of:
step 1, a certain amount of asphalt fiber is put into a non-melting reactor (5), and is sequentially connected with a mass flowmeter (1), a front constant pressure valve (2), a non-melting furnace (4), the non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) after being sealed, and N with the pressure of 3MPa is adopted 2 After the air tightness of the device is detected, the rear constant pressure valve (6) is used for emptying;
step 2, opening the mass flowmeter (1) and setting flow;
step 3, setting the pressure of a front constant pressure valve (2) and a rear constant pressure valve (6);
step 4, setting a temperature raising program of the non-melting furnace (4), turning on a heating switch, simultaneously turning on a mass spectrum (7), and setting detected charge-to-mass ratios as 44 and 18;
step 5, after the mass spectrum (7) detects that the maximum peak of the curves with the charge-mass ratios of 44 and 18 is gradually flattened, continuing to operate the heating program for 20min, and closing heating; when the temperature of the non-melting furnace (4) is reduced to room temperature, closing air, opening the front constant pressure valve (2) and the rear constant pressure valve (6) to empty the system pressure; the fiber in the unmelted reactor (5) is the unmelted fiber.
The front constant pressure valve (2) is 0.05MPa higher than the set pressure of the rear constant pressure valve (6), and the pressure setting range is 0.45-3.0 MPa.
Further, the temperature rising speed of the non-melting furnace (5) is 0.2-5 ℃/min, the final temperature is 270-310 ℃, and the final temperature residence time is 6h.
Further, the asphalt fiber is general-purpose asphalt fiber or mesophase asphalt fiber.
Compared with the prior art, the invention has the following advantages:
according to the device and the method for pressurizing the unmelted asphalt fibers, the pressurized air is adopted to unmelt the asphalt fibers, so that the unmelted reaction is promoted to right, and the oxygen is accelerated to diffuse inwards along the radial direction of the fibers, so that the unmelted time is reduced; the non-melting reaction degree is determined by adopting mass spectrum on-line detection, and the trouble of determining the non-melting degree by high-temperature sampling and weighing is avoided, so that the defects of long non-melting time and complex operation of the asphalt fiber in the prior art are overcome, and the mechanical property of the prepared asphalt fiber is hardly changed compared with that of a conventional air method.
Drawings
FIG. 1 is a schematic view of the structure of the pressurized non-melting apparatus of the present invention.
1. A mass flowmeter; 2. a front constant pressure valve; 3. a pressure sensor; 4. a non-melting furnace; 5. a non-melting reactor; 6. a rear constant pressure valve; 7. mass spectrometry
Detailed Description
Example 1
The device for pressurizing unmelted asphalt fibers is formed by sequentially connecting a mass flowmeter (1), a front constant pressure valve (2), an unmelting furnace (4), an unmelting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7). The mass flowmeter (1), the front constant pressure valve (2), the unmelted reactor (5) and the rear constant pressure valve (4) are connected by stainless steel pipes in sequence; the non-melting reactor (5) is arranged in the tubular heating furnace (4); the sample inlet of the mass spectrum (7) is arranged in the pipeline at the rear end of the rear constant pressure valve (6).
The non-melting furnace (4) is a tubular heating furnace, and a heater capable of programming temperature is arranged on the outer side of the non-melting furnace;
the unmelted reactor (5) is a stainless steel reactor, and both ends of the unmelted reactor are sealed by hard sealing;
the front constant pressure valve (2) is a YT-2 type constant pressure valve; the rear constant pressure valve (6) is a YT-4 type constant pressure valve.
Example 2
Step 1, 5g of general-purpose asphalt fiber with the softening point of 230 ℃ is put into a non-melting reactor, and sealed and then is subjected to a mass flow meter (1), a front constant pressure valve (2), a non-melting furnace (4), a non-melting reactor (5), a rear constant pressure valve (6) and massThe spectra (7) are connected in sequence, N adopting the pressure of 3MPa 2 After the air tightness of the device is detected, the device is emptied by a rear constant pressure valve;
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, setting the pressure of the front constant pressure valve and the rear constant pressure valve to be 3MPa and 2.95MPa;
step 4, setting a heating program of the non-melting furnace to be 5 ℃/min to 170 ℃, then heating to 310 ℃ at 0.2 ℃/min, keeping the temperature at 310 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum, and setting the detected charge-to-mass ratio to be 44 and 18;
step 5, after the reaction had proceeded for 729 minutes, it was found that the line of mass spectrum detectors 44 and 18 tended to be flat, and after proceeding for 749 minutes, the heating was turned off. After cooling to room temperature, the air was closed, the front constant pressure valve and the rear constant pressure valve were opened to empty the system pressure to normal pressure, and the fiber mass was weighed to be 5.49g.
Example 3
Step 1, placing 5g of general-purpose asphalt fiber with a softening point of 270 ℃ into a non-melting reactor, sealing, sequentially connecting the non-melting furnace (4), the non-melting reactor (5), a rear non-melting valve (6) and a mass spectrum (7) according to a mass flowmeter (1), a front non-melting valve (2), and adopting N with a pressure of 3MPa 2 After the air tightness of the device is detected, the device is emptied by a rear constant pressure valve;
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, setting the pressure of the front constant pressure valve and the rear constant pressure valve to be 1MPa and 0.95MPa; setting the temperature-raising program of the non-melting furnace to 5 ℃/min to 170 ℃, then raising the temperature to 290 ℃ at 0.4 ℃/min, keeping the temperature at 290 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum at the same time, and setting the detection charge-to-mass ratio to 44 and 18;
step 5, after the reaction had progressed to 509 minutes, the line of mass spectrometric detectors 44 and 18 was found to be gentle, and after proceeding to 529 minutes, the heating was turned off. After cooling to room temperature, the air was closed, the front constant pressure valve and the rear constant pressure valve were opened to empty the system pressure to normal pressure, and the fiber mass was weighed to be 5.41g.
Example 4
Step 1, 5g of mesophase pitch fiber with a softening point of 268 ℃ is put into a non-melting reactor, and after sealing, the 5g of mesophase pitch fiber is sequentially connected with a mass flow meter (1), a front constant pressure valve (2), a non-melting furnace (4), a non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) according to a mass flow meter (1), and N with a pressure of 3MPa is adopted 2 After the air tightness of the device is detected, the device is emptied by a rear constant pressure valve;
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, setting the pressure of the front constant pressure valve and the rear constant pressure valve to be 0.5MPa and 0.45MPa;
step 4, setting a heating program of the non-melting furnace to be 5 ℃/min to 170 ℃, then heating to 270 ℃ at 0.5 ℃/min, keeping the temperature at 270 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum detector, and setting the detection charge-to-mass ratio to be 44 and 18;
step 5, after the reaction had proceeded to 289 minutes, the line of mass spectrum detectors 44 and 18 was found to be gentle, and after proceeding to 309 minutes, the heating was turned off. After cooling to room temperature, the air was closed, the front constant pressure valve and the rear constant pressure valve were opened to empty the system pressure to normal pressure, and the fiber mass was weighed to 5.35g.
Example 5
Step 1, placing 5g of general-purpose asphalt fiber with a softening point of 230 ℃ into a non-melting reactor, sealing, sequentially connecting the non-melting furnace (4), the non-melting reactor (5), a rear non-melting valve (6) and a mass spectrum (7) according to a mass flowmeter (1), a front non-melting valve (2),
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, completely opening the front constant pressure valve and the rear constant pressure valve;
step 4, setting a heating program of the non-melting furnace to be 5 ℃/min to 170 ℃, then heating to 310 ℃ at 0.2 ℃/min, keeping the temperature at 310 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum detector, and setting detection charge-to-mass ratios to be 44 and 18;
step 5, after the reaction had progressed to 849 minutes, the line of mass spectrometric detectors 44 and 18 was found to flatten out, and after proceeding to 869 minutes, the heating was turned off. After cooling to room temperature, the air was turned off and the fiber mass was weighed to be 5.50g.
Example 6
Step 1, placing 5g of general-purpose asphalt fiber with a softening point of 270 ℃ into a non-melting reactor, and sequentially connecting the non-melting furnace (4), the non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) according to a mass flowmeter (1), a front constant pressure valve (2), a non-melting furnace (4) and a mass spectrum (7) after sealing;
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, completely opening the front constant pressure valve and the rear constant pressure valve;
step 4, setting a heating program of the non-melting furnace to be 5 ℃/min to 170 ℃, then heating to 290 ℃ at 0.4 ℃/min, keeping the temperature at 290 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum detector, and setting the detection charge-to-mass ratio to be 44 and 18;
step 5, after the reaction had proceeded to 599 minutes, it was found that the line of mass spectrometric detectors 44 and 18 tended to flatten, and after 629 minutes, the heating was turned off. After cooling to room temperature, the air was turned off and the fiber mass was weighed to be 5.43g.
Example 7
Step 1, 5g of mesophase pitch fiber with a softening point of 268 ℃ is put into a non-melting reactor, and is sequentially connected with a mass flowmeter (1), a front constant pressure valve (2), a non-melting furnace (4), a non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) after being sealed;
step 2, air is introduced, a mass flowmeter is opened at the same time, and the flow rate is set to be 100mL/min;
step 3, completely opening the front constant pressure valve and the rear constant pressure valve;
step 4, setting a heating program of the non-melting furnace to be 5 ℃/min to 170 ℃, then heating to 270 ℃ at 0.5 ℃/min, keeping the temperature at 270 ℃ for 6 hours, turning on a heating switch, turning on a mass spectrum detector, and setting the detection charge-to-mass ratio to be 44 and 18;
step 5, after the reaction had progressed to 339 minutes, the line of mass spectrum detectors 44 and 18 was found to be gentle, and after proceeding to 359 minutes, the heating was turned off. After cooling to room temperature, the air was turned off and the fiber mass was weighed to be 5.35g.
Table 1 shows the mechanical properties of pitch carbon fibers prepared by melting the fibers in examples 2 to 7 of the present invention
It can be seen from examples 2-7 that the use of pressurized air to infuse the pitch fibers reduces the infusibility time; on-line detection of H using mass spectrometry 2 O and CO 2 The concentration change of the asphalt fiber is used for determining the infusibility reaction degree, and the trouble of determining the infusibility degree by high-temperature sampling and weighing is avoided, so that the defects of long infusibility time and complex operation of the asphalt fiber in the prior art are overcome, and the mechanical property of the prepared asphalt fiber is hardly changed compared with that of a conventional air method.
What is not described in detail in the present specification belongs to the prior art known to those skilled in the art. While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.
Claims (7)
1. An apparatus for pressurizing unmelted pitch fibers, comprising: the device consists of a mass flowmeter (1), a front constant pressure valve (2), a non-melting furnace (4), a non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) which are sequentially connected; the mass flowmeter (1), the front constant pressure valve (2), the rear constant pressure valve (6) and the unmelted reactor (5) are connected by stainless steel pipes in sequence; the unmelted reactor (5) is arranged in the unmelted furnace (4); a sample inlet of the mass spectrum (7) is arranged in a pipeline at the rear end of the rear constant pressure valve (6); the non-melting furnace (4) is a tubular heating furnace, and a heater capable of programming temperature is arranged on the outer side of the non-melting furnace; the non-melting reactor (5) is a stainless steel reactor, and both ends of the non-melting reactor are sealed hard.
2. An apparatus for pressurizing unmelted pitch fibers as recited in claim 1, wherein: the front constant pressure valve (2) is used for controlling the pressure of a rear device of the front constant pressure valve to be a constant value; the rear constant pressure valve (6) is used for controlling the pressure of a front device to be a constant value.
3. An apparatus for pressurizing unmelted pitch fibers as recited in claim 1, wherein: the front constant pressure valve (2) is a YT-2 type constant pressure valve; the rear constant pressure valve (6) is a YT-4 type constant pressure valve.
4. A method of unmelting pitch fibers using a pressurized unmelting pitch fiber apparatus as defined in claim 1, wherein: the method comprises the following steps:
step 1, a certain amount of asphalt fiber is put into a non-melting reactor (5), and is sequentially connected with a mass flowmeter (1), a front constant pressure valve (2), a non-melting furnace (4), the non-melting reactor (5), a rear constant pressure valve (6) and a mass spectrum (7) after being sealed, and N with the pressure of 3MPa is adopted 2 After the air tightness of the device is detected, the rear constant pressure valve (6) is used for emptying;
step 2, opening the mass flowmeter (1) and setting flow;
step 3, setting the pressure of a front constant pressure valve (2) and a rear constant pressure valve (6);
step 4, setting a temperature raising program of the non-melting furnace (4), turning on a heating switch, simultaneously turning on a mass spectrum (7), and setting detected charge-to-mass ratios as 44 and 18;
step 5, after the mass spectrum (7) detects that the maximum peak of the curves with the charge-mass ratios of 44 and 18 is gradually flattened, continuing to operate the heating program for 20min, and closing heating; when the temperature of the non-melting furnace (4) is reduced to room temperature, closing air, opening the front constant pressure valve (2) and the rear constant pressure valve (6) to empty the system pressure; the fiber in the unmelted reactor (5) is the unmelted fiber.
5. The method of unmelting asphalt fibers of claim 4, wherein: the front constant pressure valve (2) is 0.05MPa higher than the set pressure of the rear constant pressure valve (6), and the pressure setting range is 0.45-3.0 MPa.
6. The method of unmelting asphalt fibers of claim 4, wherein: the temperature rising speed of the non-melting furnace (4) is 0.2-5 ℃/min, the final temperature is 270-310 ℃, and the final temperature residence time is 6h.
7. The method of unmelting asphalt fibers of claim 4, wherein: the asphalt fiber is general-purpose asphalt fiber or mesophase asphalt fiber.
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| CN202211287381.7A CN115434043B (en) | 2022-10-20 | 2022-10-20 | Device and method for pressurizing and not melting asphalt fibers |
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| CN115434043B true CN115434043B (en) | 2024-02-06 |
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| CN112064340A (en) * | 2020-09-14 | 2020-12-11 | 湖南东映碳材料科技有限公司 | Quasi-isotropic high-thermal-conductivity composite material and preparation method thereof |
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| CN113686945A (en) * | 2021-07-23 | 2021-11-23 | 长安大学 | Rapid analysis and detection system and method for volatile organic compounds in asphalt flue gas |
| CN114790592A (en) * | 2022-02-15 | 2022-07-26 | 武汉科技大学 | Method for preparing high-performance asphalt-based carbon fiber through rapid pre-oxidation |
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| AU2016383457A1 (en) * | 2015-12-29 | 2018-07-12 | Centre National De La Recherche Scientifique (Cnrs) | Method for detecting and quantifying oxygen in oxidizable compounds |
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